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EP0460110B1 - Procede de recuperation en continu de gaz de fluorure d'hydrogene - Google Patents

Procede de recuperation en continu de gaz de fluorure d'hydrogene Download PDF

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Publication number
EP0460110B1
EP0460110B1 EP90905159A EP90905159A EP0460110B1 EP 0460110 B1 EP0460110 B1 EP 0460110B1 EP 90905159 A EP90905159 A EP 90905159A EP 90905159 A EP90905159 A EP 90905159A EP 0460110 B1 EP0460110 B1 EP 0460110B1
Authority
EP
European Patent Office
Prior art keywords
stream
hydrogen fluoride
dehydrating
accordance
sulfur trioxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP90905159A
Other languages
German (de)
English (en)
Other versions
EP0460110A1 (fr
Inventor
Henry Buehler
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mallinckrodt Inc
Original Assignee
Mallinckrodt Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mallinckrodt Inc filed Critical Mallinckrodt Inc
Publication of EP0460110A1 publication Critical patent/EP0460110A1/fr
Application granted granted Critical
Publication of EP0460110B1 publication Critical patent/EP0460110B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/19—Fluorine; Hydrogen fluoride
    • C01B7/191—Hydrogen fluoride
    • C01B7/195—Separation; Purification
    • C01B7/196—Separation; Purification by distillation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/19—Fluorine; Hydrogen fluoride
    • C01B7/191—Hydrogen fluoride
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/38—Separation; Purification; Stabilisation; Use of additives
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Definitions

  • the aqueous heel is pumped via inlet line 5 into holding tank 10.
  • the heel will most often be a by-product of another process, the invention is not so limited.
  • the heel is received into the holding tank at a temperature above 0 °C. This 0 °C temperature limitation is desired to avoid the possibility of the alkali metal fluoride precipitating out of solution.
  • the heel is then maintained within holding tank (10) at a temperature between 0 and 40 °C, preferably between 25 and 40 °C and most preferably between 35 and 40 °C.
  • the sulfur-containing stream will be combined with the heel so as to provide a ratio of 0.8 to 0.9, and more preferably 0.81 to 0.84, moles of SO3 per mole of water.
  • the volume of the stream can then vary with the strength of the oleum (% SO3 in H2SO4) and the percent water in the heel to be treated.
  • Substantially anhydrous hydrogen fluoride is condensed within the condenser (40).
  • the remaining portion of the mixed stream cascades down through the heat recovery tower (30) while high temperature (100 to 190 °C, preferably 125 to 155 °C) hydrogen fluoride vapor is passed upwards through the tower.
  • high temperature (100 to 190 °C, preferably 125 to 155 °C) hydrogen fluoride vapor is passed upwards through the tower.
  • the falling mixed stream and rising hydrogen fluoride vapor reach thermal equilibrium within the tower whereupon additional hydrogen fluoride gas (nominally about fifty to sixty percent of the original hydrogen fluoride content of the mixed stream) evaporates.
  • the hydrogen fluoride gas rises through the heat recovery tower and is separated along with the initial hydrogen fluoride portion for transport to the condenser (40).
  • the residence time within this reactor is adjusted so that the residual hydrogen fluoride can be distilled off and the alkali metal bifluoride can be converted to two moles of hydrogen fluoride and subsequently recovered.
  • the hydrogen fluoride gas separated within the high temperature reactor (50) is utilized as the countercurrent, high temperature hydrogen fluoride gas stream within the heat recovery tower. The efficiency of the process is enhanced by supplying heat recovered from within the tower (30) to the underflowing reactor vessel (50).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

Un procédé de récupération en continu de gaz de fluorure d'hydrogène anhydre consiste à mettre en contact une solution aqueuse d'un fluorure de métal alcalin dans de l'acide fluorique avec un courant de déshydratation contenant du soufre. Le courant de déshydratation consiste de préférence en du trioxyde de soufre dissous dans de l'acide sulfurique. Le produit désiré est obtenu en grande quantité et pureté.

Claims (11)

  1. Procédé pour la production en continu de fluorure d'hydrogène gazeux qui comprend :
    a. la mise en contact d'un courant aqueux d'acide fluorhydrique contenant un fluorure de métal alcalin avec un courant déshydratant contenant du soufre, formant ainsi un courant mélangé;
    b. l'introduction du courant mélangé dans la partie supérieure d'une tour de récupération de chaleur, provoquant ainsi l'émission de fluorure d'hydrogène gazeux à partir du courant mélangé;
    c. le passage du courant mélangé à travers la tour de récupération de chaleur tout en mettant en contact le courant mélangé avec un flux à contre-courant constitué de fluorure d'hydrogène gazeux chauffé, provoquant ainsi l'émission de fluorure d'hydrogène gazeux supplémentaire du courant mélangé;
    d. le passage du courant mélangé de la tour de récupération de chaleur dans un récipient réactionnel à haute température ; et
    e. le chauffage du courant mélangé dans le récipient pour provoquer encore l'émission de fluorure d'hydrogène gazeux à partir du courant mélangé.
  2. Procédé selon la revendication 1, dans lequel ledit fluorure d'hydrogène gazeux supplémentaire qui est émis à partir du courant mélangé pendant l'étape de passage est transporté à travers une tour de distillation.
  3. Procédé selon la revendication 1, dans lequel ledit courant déshydratant contient de l'acide sulfurique.
  4. Procédé selon la revendication 3, dans lequel ledit courant déshydratant contient de plus du trioxyde de soufre.
  5. Procédé selon la revendication 4, dans lequel ledit courant de déshydratation comprend d'environ 20 à environ 90% de trioxyde de soufre dans de l'acide sulfurique (pour-cent veut dire parties de trioxyde de soufre par rapport aux parties d'acide sulfurique à 100 %).
  6. Procédé selon la revendication 4, dans lequel ledit courant déshydratant comprend d'environ 65 à environ 80 % de trioxyde de soufre dans de l'acide sulfurique.
  7. Procédé selon la revendication 4, dans lequel ledit courant déshydratant comprend environ 65 % de trioxyde de soufre dans de l'acide sulfurique.
  8. Procédé selon la revendication 1, dans lequel ledit fluorure de métal alcalin est choisi entre le fluorure de sodium et le fluorure de potassium.
  9. Procédé selon la revendication 4, dans lequel ladite étape de mise en contact comprend la mise en contact dudit courant aqueux avec une quantité dudit courant déshydratant correspondant à environ 0,8 à 0,9 mole de trioxyde de soufre dans ledit courant déshydratant par mole d'eau dans ledit courant aqueux.
  10. Procédé selon la revendication 4, dans lequel ladite étape de mise en contact comprend la mise en contact dudit courant aqueux avec une quantité dudit courant déshydratant correspondant à environ 0,81 à 0,84 mole de trioxyde de soufre dans ledit courant déshydratant par mole d'eau dans ledit courant aqueux.
  11. Procédé selon la revendication 4, dans lequel ladite étape de mise en contact comprend la mise en contact dudit courant aqueux avec une quantité dudit courant déshydratant correspondant à environ 0,83 mole de trioxyde de soufre dans ledit courant déshydratant par mole d'eau dans ledit courant aqueux.
EP90905159A 1989-02-27 1990-02-22 Procede de recuperation en continu de gaz de fluorure d'hydrogene Expired - Lifetime EP0460110B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US31550389A 1989-02-27 1989-02-27
US315503 1989-02-27
US07/376,572 US5032371A (en) 1989-02-27 1989-07-07 Process for the continuous recovery of hydrogen fluoride gas
US376572 1989-07-07

Publications (2)

Publication Number Publication Date
EP0460110A1 EP0460110A1 (fr) 1991-12-11
EP0460110B1 true EP0460110B1 (fr) 1994-02-02

Family

ID=26979937

Family Applications (1)

Application Number Title Priority Date Filing Date
EP90905159A Expired - Lifetime EP0460110B1 (fr) 1989-02-27 1990-02-22 Procede de recuperation en continu de gaz de fluorure d'hydrogene

Country Status (6)

Country Link
US (1) US5032371A (fr)
EP (1) EP0460110B1 (fr)
JP (1) JPH04503658A (fr)
AU (1) AU5330590A (fr)
DE (1) DE69006489T2 (fr)
WO (1) WO1990009957A1 (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0686136B1 (fr) * 1993-02-24 1999-08-11 E.I. Du Pont De Nemours And Company Procede ameliore de fabrication d'aromates fluores
US5744116A (en) * 1994-12-08 1998-04-28 Cameco Corporation Reaction of uranium fluorides with mineral acids to recover hydrogen fluoride
ES2155201T3 (es) 1995-10-10 2001-05-01 Ici Plc Procedimiento para la recuperacion de fluoruro de hidrogeno.
US5632966A (en) * 1996-03-07 1997-05-27 Alliedsignal Inc. Process for hydrogen fluoride separation
US5766483A (en) * 1996-05-10 1998-06-16 Alliedsignal Inc. Process for hydrogen fluoride separation
GB9707176D0 (en) * 1997-04-09 1997-05-28 Ici Plc Hydrogen fluoride recovery process
US20070098624A1 (en) * 2005-10-27 2007-05-03 Honeywell International Inc. Andhydrous hydrogen fluoride composition and method of producing the same
KR20220028073A (ko) * 2019-08-30 2022-03-08 쇼와 덴코 가부시키가이샤 불소 가스의 제조 방법
CN112047302B (zh) * 2020-08-25 2021-10-19 福建天甫电子材料有限公司 一种用于电子级氢氟酸的制备装置及制备工艺
CN114146586B (zh) * 2021-12-30 2023-11-21 金宏气体股份有限公司 一种氢氟酸溶液的配置装置及方法
CN116216647B (zh) * 2022-12-31 2024-09-17 福建舜跃科技股份有限公司 含水氢氟酸利用多段硫酸解析法制备无水氟化氢绿色方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2939766A (en) * 1957-07-01 1960-06-07 Olin Mathieson Method of producing hydrogen fluoride
DE2543965C3 (de) * 1975-10-02 1981-07-09 Bayer Ag, 5090 Leverkusen Verfahren zur Reinigung von Reaktionsgasen der Flußsäureherstellung
US4120939A (en) * 1977-05-26 1978-10-17 E. I. Du Pont De Nemours And Company Hydrogen fluoride process
FR2586247B1 (fr) * 1985-08-19 1987-11-20 Rhone Poulenc Spec Chim Procede de preparation de composes aromatiques fluores
GB2198722B (en) * 1986-12-22 1991-04-17 Comalco Alu Process for the recovery of fluoride values

Also Published As

Publication number Publication date
DE69006489T2 (de) 1994-05-11
JPH04503658A (ja) 1992-07-02
DE69006489D1 (de) 1994-03-17
US5032371A (en) 1991-07-16
EP0460110A1 (fr) 1991-12-11
WO1990009957A1 (fr) 1990-09-07
AU5330590A (en) 1990-09-26

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